Properties of tablet influenced by compression

• Higuchi and Train were probably the first pharmaceutical

scientists to study the effect of compression on tablet
characteristics ( density, disintegration, hardness, porosity,
and specific surface ) and on distribution of pressure.
– The relationship between applied pressure and weight,
thickness, density, and the force of ejection are relatively
independent of the material being compressed .
– Hardness, tensile strength, friability, disintegration, and
dissolution are properties that depend predominately on
the formulation.
• However, the developmental scientist should realize that
processing and formulation are integrated disciplines, and
the effect of one on a pharmaceutical product can not be
totally separated from the other.

1.Density and porosity:

 The apparent density of a tablet is the quotient of the weight and
the geometric volume. The apparent density of a tablet is
exponentially related to the applied pressure (or compressional
force), as shown in Figure 2, until the limiting density of the material is
approached .
 As shown in Figure 7, a plot of the apparent density against the
logarithm of applied pressure is linear except at high pressures.
 As the porosity and apparent density are inversely proportional, the
plot of porosity against the logarithm of applied pressure is linear
with a negative slope, as shown in Figure 8.
 When equal weights of aspirin and lactose are compressed with 10%
starch, the porosity of the lactose-aspirin tablet, as indicated in Figure
8, is of a magnitude between that of the individual lactose and
aspirin tablets at corresponding pressure. Thus, in tablet formulation
it may be anticipated that a change in percent composition will have a
corresponding arithmetic (or averaging) effect on porosity and
apparent density.
1.Density and porosity:

Figure 2
The eff ect of
applied pressure
on the apparent
density of tablets
of sulfathiazole
Figure 7
The eff ect of applied
pressure on the
apparent density of
sulfathiazole tablets.

Figure 8
The eff ect of
applied
pressure on the
porosity of
various tablets

2. Hardness and Tensile strength:

 The ability of a tablet to withstand mechanical handling and transport has
been evaluated by various types of tests (abrasion, bending, indentation,
hardness, diametral crushing). Although hardness is not a fundamental
property, diametral crushing is most frequently used for inprocess control
because of its simplicity.
 There is a linear relationship between tablet hardness and the logarithm
of applied pressure except at high pressures. As shown in Figure 9 for
lactose-aspirin tablets, compressed mixtures have hardness values
between those of tablets composed of the individual ingredients.
 The strength of a tablet may be expressed as a tensile strength
(breaking stress of a solid unit cross section in kg /cm 2 ).
 As shown in Figure 10, the radial tensile strength is proportional to the
applied pressure.
 For an isotropic, homogeneous tablet, the radial and axial tensile
strengths are equal. In practice the distribution of pressure, differences in
density within the tablet, and the mixture of several ingredients
contribute to the nonhomogeneity of the tablet and to the
nonuniformity of tensile strength.
2. Hardness and Tensile strength:
 When a brittle material is compressed axially, the stress upon each particle
does not necessarily compress the particles along the axial direction because
of random packing and alignment of the particles toward each other during
the events of compression.
 A greater probability exists for vertical stress on the particles during the
arrangement and fragmentation events due to the movement of the
punch.
 The overall result is that more clean surfaces are created when they are
normal to the radial direction. As applied pressure is increased,
fragmentation results in a stronger, radial tensile strength than axial
tensile strength as shown in Figure 10.
 If more bonds are formed in the radial direction, the potential for the
presence of cracks or dislocations is greater in the axial than in the radial
direction.

2. Hardness and Tensile strength:

Figure 10
Figure 9 The eff ect of applied pressure
The eff ect of applied pressure on on tensile strengths of
the hardness of various tablets tablets of dibasic calcium
phosphate dihydrate
granulated with 1.2% starch.
At each applied pressure,
the value is given for σz/σx.
2. Hardness and Tensile strength: (Radial and axial tensile strength)

 The radial tensile strength σ x is determined by a diametral compression test in

which the maximum force F σ to cause tensile failure (fracture) is measured.
The radial tensile strength is then calculated by

in which D is the diameter, and t is the thickness of the tablet.

 The axial tensile strength is determined by measurement of the maximum

force F σ to pull the tablet apart in tensile failure. The axial tensile strength is
then calculated by

2. Hardness and Tensile strength: (Radial and axial tensile strength)

 A blend of powders may be granulated with a granulating solution to increase
the adhesiveness of a formulation.
 The influence of the concentration of povidone on the tensile strengths of
hydrous lactose is shown in Figure 11. The radial strength is little effected
by the concentration of povidone, but the axial tensile strength is
increased by increased concentrations of povidone to a strength greater
than the radial strength.
 The influence of applied pressure on the tensile strengths of lactose with
1 and 9% povidone is shown in Figure 12.
 The relationship of the crushing strength of granulations of lactose with
povidone to the axial and radial tensile strengths of tablets compressed at
890 kg /cm 2 from the granulations is shown in Figure 13. The tensile
strengths of the tablet are increased as the resistance to crushing of the
granules is increased. The strength of the granule is increased as the
concentration of the binder is increased; thus, the effect of the strength
of the granule on the tensile strengths of the tablet is inseparable from
the effect of concentration. Although the crushing strength of granules is
important in the handling of the granulation in the tableting process, the
applied pressure and the concentration of the binder determine the
tensile strengths of a tablet.
 2. Hardness and Tensile strength: (Radial
and axial tensile strength)

Figure 11 Figure 1 2
Th e effect of povidone on the Th e effect of applied
tensile strengths of tablets of pressure on the tensile
hydrous lactose compressed at strengths of tablets of
8 9 0 kg/cm 2 . At each applied hydrous lactose
pressure the value is given for granulated with 1 % (__)
σ z /σ x . a n d 9 % (- - - - - -)
povidone.

Figure 1 3 Relationship of binder concentration to grnule strength an d tensile strengths of

tablets compressed at 8 9 0 kg /c m 2 from lactose monohydrate granulated with povidone. (
) granule strength, ( ) axial,
and ( ) radial tensile strength

2. Hardness and Tensile strength: (Radial and axial tensile strength)

 With a hardness tester of the diametral compression type, weak tablets tend
to fail due to tensile stresses, and strong tablets tend to fail due to
compressive stresses.
 Hardness is proportional to radial tensile strength. As shown in Figure 14,
the relationship of hardness to axial tensile strength is nonlinear. As the
hardness is increased, at higher values of hardness, there is a progressive
lessening of the rate of increase of the axial tensile strength until a
limiting axial tensile strength is attained. Thus, if the mechanical strength
of a tablet is considered only in terms of its hardness, nothing is known of
its axial strength; and if the axial tensile strength were weak, the tablet
would laminate under stress.
Figure 1 4
Th e relationship of hardness an d
axial tensile strength for dibasic
calcium phosphate dihydrate with
various concentrations of
m ag n esiu m stearate. (

) 0% , (

) 0.07 5%, (

) 0.12 5%, (

) 0.25 %,
(
3. Specific Surface:
 Specific surface is the surface area of 1 g of
material. The influence of applied pressure on the
specific surface area of a tablet is typified by Figure
15.
As the lactose granules, which were
granulated by adding 10% starch paste, are
compressed, the specific surface is increased to a
maximal value (four times that of the initial
granules), indicating the formation of new
surfaces due to fragmentation of the granules.
 Further increases in applied pressure produce a
progressive decrease in specific surface as
 the particles bond. Figure 15
A similar relation is shown for aspirin containing 10% starch.
When a equal weight of aspirin and lactose is blended with The effect of applied
10% starch and then compressed, the specific surface is pressure on the
between that of the aspirin and lactose tablets individually. As specific surface of
the relationship between applied pressure and apparent
density is independent of the material being compressed, the various tablets
influence of starch on the specific surface and porosity is not
significant. For these aspirin, lactose, and aspirin-lactose
tablets, the maximum specific surface occurs at a porosity of
approximately 10%, even though the applied pressures at
which the maxima occur vary with the different materials.

4. Disintegration:
 Usually, as the applied pressure used to prepare a tablet is increased, the
disintegration time is longer. Frequently, there is an exponential relationship
between the disintegration time an d the applied pressure, as s h o wn for aspirin an d
lactose in Figure 16.
 In other formulations there is a mi n i mu m value wh en the applied pressure is
plotted against the logarithm of disintegration time, as s h o wn in Figures 1 6 a n d
1 7 with 1 0 % starch.
 F o r tablets co mpressed at l o w pressures, there is a large void, an d the contact of starch
grains in the interparticular space is discontinuous. Thus, there is a lag time before the starch
grains, wh i ch are swelling d u e to imbitition of water, contact a n d exert a force on the
surrounding tablet structure.
 F o r tablets co mpressed at a certain applied pressure, the contact of the starch grains
is continuous with the tablet structure, a n d the swelling of the starch grains immediately
exerts pressure, causing the mo st rapid disintegration, as demonstrated b y a m i n i m u m in
a plot of applied pressure against the logarithm of disintegration time.
 F o r tablets co mpressed at pressures greater tha n that pro ducing the m i n i m u m
disintegration time , the porosity is such that m o re time is required for the penetration of
water into the tablet, with a resulting increase in disintegration time.
 As s h o w n in Fig ure 1 7 for sulfadiazine tablets, the concentration of a disintegrating agent
influences the relationship between applied pressure a n d disintegration time. For lo w
starch concentrations, a small ch an g e in the applied pressure causes a large ch an g e in
disintegration time. Th us, for formulations containing a small percent of starch,
fluctuations in applied pressure during tablet production cause a large variance in
disintegration time.
 4. Disintegration:

Figure 16 Figure 17
The eff ect of applied pressure on The eff ect of applied pressure
disintegration time of various on the disintegration time of
tablets. sulfadiazine tablets with
various percentages of dried
corn starch.

5. Dissolution :
 T h e effect of applied o n dissolution rate m ay b e
pressure
considered from viewpoint of disintegrating a n d non-
disintegrating tablets.
• S h a h & Parrot s h o we d that, the dissolution rate is independent
of applied pressure from 53 to 2 1 7 0 kg /cm 2 for non-
disintegrating spheres of aspirin, benzoic acid, salicycic acid, a n
equimolar mix.of aspirin & salicylic acid, aspirin & caffeine .
 Mitchell a n d Savill found dissolution rate of aspirin disk to
b e independent of pressure over 2 0 0 0 -13000 kg /cm 2 a n d
independent of particle size of granules u se d to prepare
benzoic disks.
 Kanke a n d Sekiguchi [32] reported that the dissolution rate
of benzoic acid disks is independent of particle size a n d
applied pressure.
 • The effect of applied pressure on dissolution of disintegrating tablet is
difficult to predict. ; however, for a conventional tablet it is dependent on the
pressure range, the dissolution medium, and the properties of the medicinal
compound and the excipients.
 If fragmentation of the granules occurs during compression, the
dissolution is faster as the applied pressure is increased, and the
fragmentation increases the specific surface.
 If the bonding of the particles is the predominate phenomena in
compression, the increase in applied pressure causes a decrease in
dissolution.
The four most common dissolution-pressure relations are:
1. The dissolution is more rapid as the applied pressure is increased.
2. The dissolution is slowed as the applied pressure is increased.
3. The dissolution is faster, to a maximum, as the applied force is increased,
and then a further increase in applied pressure slows dissolution.
4. The dissolution is slowed to a minimum as the applied pressure is increased,
and then further an increase in applied pressure speeds dissolution.

Th e complexity of the release of a medicinal co mp o u n d from a tablet is demonstrated

in Table 1 for sulfadimidine tablets prepared b y wet granulation using three different
granulating agents .
• W h e n starch paste was used as the granulating agent, dissolution was faster as the
applied pressure was increased.
•W h e n a methylcellulose solution was used as the granulating agent, dissolution
was
slowed as the applied pressure was increased.
•W h e n a gelatin solution was used as a granulating agent, the dissolution became
faster as the applied pressure was increased to a maximum, and then further increases
in applied pressure slowed dissolution.
t 5 0 % (min)
Pressure Starch paste Methylcellulose Gelatin solution
(MN/cm2) solution

200 54.0 0.5 10.0

400 42.0 0.8 4.5
600 35.0 1.1 3.0
800 10.0 1.2 4.6
1000 7.0 1.4 4.9
2 0 0 0 1: Eff ect of3.3
Table compressional 1.8
force 6.5
on dissolution
of Sulfadimide tablets prepared with various
garnulating agents
 Forces involved in compression
Forces, which influence the compaction of granules.

Force distribution:
 The fundamentals of tabletting have been carried out on
single- station press or even on isolated punch & punches with
hydraulic press.
 When force is being applied to top of a cylindric powder mass, the
following basic relationship applies, since there must be an axial
(vertical) balance of forces.
 the system is represented diagrammatically .
FA = FL + F D
Where,
F A = force applied to upper punch
F L = proportion of F A force transmitted to lower punch,
F D =reaction at the die wall due to friction at the surface
• Because of this inherent difference between the force applied at the upper
punch & that affecting material close to the lower punch, a mean compression
force applied is given by :
F M = FA + F L
2
• Fm gives practically friction independent measure of compaction load which is
more relevant than FA .
• In single station press applied force transmission decays exponentially (i.e. F
L = FA .e – k h /d )to over come this, appropriate geometric force F G might be used,
F G = FA x F L

Use of these parameters are more appropriate than F A when determining

relationship b/w compression force and tablet properties like tablet strength.
 Development of radial force ( F R )
 As the compression force is increased and any repacking of the tabletting
mass is completed, the material may be regarded to some extent as a
single solid body.
 Wh en compressive force is applied in one direction (vertical) results in
the decrease in height Δ (H) butni eacs of neu
dnocnfidso
il bod
,yhsti w
doulbe H) but in case of unconfined solid
body, this would be accompanied by an expansion in the horizontal
direction of ΔH) butni eacs of neu
dnocnfidso
il bod
,yhsti w
doulbe D. The ratio of these two dimensional changes
is known as poission ratio(λ) of hte ) of the material, defined as:

λ) of hte = ΔH) butni eacs of neu

dnocnfidso
il bod
,yhsti w
doulbe D/ΔH) butni eacs of neu
dnocnfidso
il bod
,yhsti w
doulbe H
 The Poisson ratio is characteristic constant for each tablet.
 Under the condition like compression the material is not free to expand in
horizontal plane bcoz its confined to die. Consequently, a radial die -wall
force F R develops perpendicular to die wall surface.
 Material with high Poisson ratio give higher F R value.
 Classical friction theory can be applied to obtain a relationship
between axial frictional force F D and radial force F R as;
F D =µ w .F R
where, µ w is coeff. of die wall friction .
 Frictional effect represented by, µ w arises from shearing of adhesions
that occurs as the particles slide along the die wall. Its magnitude is
related to shear strength S and effective area of cntct A e between two
surfaces.
 Force transmission is maxm when F D is minimum which is achieved by
adequate lubrication of die wall(lower S) and maintaining minm tablet
ht.(reducing A e ).
 Degree of lubrication is compared to measure F A &F D and determine
ratio of F L /F A. This is called the coeff. of lubrication efficeincy or R
value.
 It approaches1 for perfect lubrication, and in practice as high as 0.98
may be achieved.Values below0.8 indicate poor lubrication .

Ejection forces
 Radial die forces & die wall friction also affect the ease with which the
compressed tablet can be removed from the die. The force necessary to
eject a finished tablet follows a distintictive pattern of three stages.

 The first stage involves distinctive peak force required to initiate ejection,
by breaking of tablet/die wall adhesions.
 A smaller force usually follows, that is required push the tablet up the
die wall.
 The final stage is marked by a decline in force of ejection as the tablet
emerges from the die.

 Variation on this pattern are sometimes found when lubrication is

inadequate and/or “slip-stick” conditions occur b/w tablet and die wall.
 Worn dies, which cause the bore to become barrel shaped gives rise
abnormal ejection force and may lead to failure of tablet structure.
 A direct connection exists b/w F D and force required to eject tablet from
die, F E . For eg.well lubricated system(large R value) have been shown to
have smaller F E values.
 Compaction profiles

Many attempts have been made to minimize the amount of applied

force transmitted radially to the die walls. All such investigations lead to
characteristic hysteresis curves called as compaction profiles . Radial
pressure is developed due to the attempt of material to expand
horizontally. The plot of radial pressure against axial pressure leads to
hysteresis curve called as compaction profile .
When the elastic limit of the material is high, elastic deformation may
make the major contribution, and on removal of the applied load, the
extent of the elastic relaxation depends on the value of the material’s
modules of elasticity (young’s modulus). Lower the modulus higher will be
the elastic relaxation . Then there will be the danger of structural failure.
Higher the modulus value results in low decompression hence lesser risk of
structural failure.

Dotted line O to A represents

a high ly variable
pressure→

response
repacking, while dueat A, to D
< C
R adial

elastic
deformation becomes dominant
and continues until elastic limit
B is reached.
 F rom B to point of
m axm
com pression C , deform ation is E
B
predominantly plastic, or C’
brittle
fracture is taking A

place.
The decompression process C O
D to is accom panied b y Axial pressure
→
elastic
recovery, and if a second yield
point • The area of hysteresis loop (OABC ’)
(D) is reached, by indicates the extent of departure
plastic from ideal elastic behavior, since for a

deformation or brittle line
The decompression fracture
B to perfectly elastic body, line BC ’ would
D to represents
C’ E. the behavior of coincide with AB.
largely elastic material.
 FACTORS AFFECTING STRENGTH O F TABLETS

 The ability of a tablet to withstand mechanical handling

and transport has been evaluated by various types of tests
(abrasion, bending, idention , hardness, diametral crushing).
 The strength of a tablet may be expressed as a tensile strength
(breaking stress of a solid unit in kg /cm 2 ).

 Factors affe ctin g tablet strength are

I. Particle size
II. Moisture content
III. Lubricants
IV. Applied pressure

1.Particle size: -
• A decrease in particle size resulted in the increase in the tablet strength.
• Very large particle often exists as agglomerates of small crystal on
compression such agglomerates , being more friable than the crystal,
breakdown in smaller units. The strength of the tablets prepared from such
aggregates is higher.
• With very fine particle , such as those produced by a fluid energy mill , the
powder are very cohesive even in the uncompressed state. On
compaction strong compact of tablet can be formed .
• At a given pressure the use of a very small particle increases the chances
of grapping & the volume of air entrapped also increases.
• General equation formed for the effect of particle size is
F c = K a /√d
• Where, K= constant
a= material
constant
lies
between
(0.2 to
0.47)
Fc= hardness of the impact
d= diameter of the granule
 2. Moisture content:-
• In the preparation of the pharmaceutical tablet , it is generally
accept that a small proportion of the moisture is present and in
some cases this is required to form a coherent tablets.
• Wet granulation of the powder material with hydrophilic additive
was shown to yield tablet whose mechanical strength is
dependant on the optimum content above or below with the
tablets strength was reduced
• With the optimum moisture content there
is : Die wall lubrication
Inter-particulate lubrication
Hydro-dynamic resistance to consolidation
Expression of intestinal liquid to the die wall

• At low moisture content: ↑ e d die wall friction due to ↑ e d stress

ratio, poor tablet hardness.
• At high moisture content: moisture acts as lubricant , hence
↓ e d die wall friction
• At further ↑s e in moisture content: Further ↑s e in moisture,
↓s e in compact strength due to ↓s e in interparticulate bond.

• Hence a granulation should contain an optimum moisture

content.
• It has been reported that the optimum moisture content for
starch granulation of lactose is approximately 12% and that of
phenacetin is 3%.
 3. Lubricants
• The chief purpose of a lubricant is to minimize friction at die wall,
although they often enhances flow of granules by decreasing inter-
particular friction .
• Lubrication mechanism: The polar portion of lubricant adhere to
oxide-metal surface and interpose a film of low shear strength at
interface b/w die wall and tablet.
• A lubricant reduces ejection force.
• Although a lubricant is added to facilitate its process of tableting, its
presence affects several properties of tablet.
• The effect of lubricant on mechanical strength of tablet depends on
mechanism of bonding.
• The strongest bonds are formed b/w clean, new surface; and for
material that undergo plastic and/or elastic deformation . In such
cases lubricants acts as a physical barrier b/w new surface. Hence
strength decreases.

 Eg. A tablet of MCC, whose bonding occurs primarily through plastic

deformation and flow, is mechanically weakened by lubricant. The
addition of Mag.stearate markedly decrease axial and tensile
strength in MCC as well as Lactose tablet.
 For materials that are brittle and fragment, new, clean surfaces
are formed and readily bond during compression, and the
lubricant has little detrimental effect on strength of tablets.
 Dibasic calcium phosphate dihydrate is consolidated by brittle
fraction, and its axial and radial tensile strength are not significantly
changed by addition of as much as 3% of mag.stearate.
 Stearic acid, hydrogenated veg.oil, talc and PEG 4000 may be used
in concn as great as 8% for brittle material with only a slight to
moderate change in tensile strength.
 4. Effect of applied pressure
• At higher forces due to fragmentation new surfaces are
formed causing an increase in surface area, hence more area
is available for bond formation, hence more will be the
hardness of the compact.
• There is a linear relationship b/w tablet hardness and the
logarthim of applied pressure except at high pressures.
• According to Balshin eqn.
Fc = Fc 0 V r - m
Where,
Fc0 = strength of the tablet when Vr =1 (i.e. completely
consolidated)
m = is a constant for particular system

Vr is the relative volume defined as Vr = 1/1 -ε

Where ε is the porosity of the compact
• And, shotton and Ganderton gave a general equation for the
effect of applied pressure on the strength of the compact.
Log P = nF c + C
Where, P= applied pressure
F c = strength of the
compact C= constant
When we extraplot the plot of logP vs F c , the intercept gives
the value of C, which probably represents the minimum
pressure required for the formation of tablet.
 Vr is the relative volume defined as Vr = 1/1 -ε
Where ε is the porosity of the compact
• And, shotton and Ganderton gave a general equation for the
effect of applied pressure on the strength of the compact.
Log P = nF c + C
Where, P= applied pressure
F c = strength of the
compact C= constant
When we extraplot the plot of logP vs F c , the intercept gives
the value of C, which probably represents the minimum
pressure required for the formation of tablet.
 Vr is the relative volume defined as Vr = 1/1 -ε
Where ε is the porosity of the compact
• And, shotton and Ganderton gave a general equation for the
effect of applied pressure on the strength of the compact.
Log P = nF c + C
Where, P= applied pressure
F c = strength of the
compact C= constant
When we extraplot the plot of logP vs F c , the intercept gives
the value of C, which probably represents the minimum
pressure required for the formation of tablet.

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